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Dimethyl Sulfoxide → HCID 21280950, 화합물

HRID 462558
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HRID 462558 반응식
[CH3:1][S:2]([CH3:5])(=[O:4])=[O:3].[H-].[Na+].CS(C)=O.C[O:13][C:14](=O)[C:15]1[CH:20]=[C:19]([CH3:21])[C:18]([N:22]([CH3:24])[CH3:23])=[C:17]([CH3:25])[CH:16]=1>C(O)(=O)C.O>[CH3:24][N:22]([CH3:23])[C:18]1[C:17]([CH3:25])=[CH:16][C:15]([C:14](=[O:13])[CH2:1][S:2]([CH3:5])(=[O:4])=[O:3])=[CH:20][C:19]=1[CH3:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 679Dimethyl SulfoxideHCID 6213Dimethyl SulfoneHCID 24758Sodium hydrideHCID 143324N,N,2,6-Tetramethylaniline-4-carboxylic acid, methyl ester

생성물 1

HCID 21280950HCID 21280950, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 962
Water
용매

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온도
80 °C

실험 절차

A suspension of 24.5 g. of dimethylsulfone and 9.1 g. of sodium hydride (50% dispersion in oil) in 50 ml. of absolute dimethylsulfoxide was stirred at 50° C. under an atmosphere of nitrogen and the exclusion of moisture for 3 hours. Then, it was treated with 16 g. of 4-(dimethylamino)-3,5-dimethyl-benzoic acid methyl ester. The mixture was stirred at 80° C. for 45 minutes, cooled and dissolved in 300 ml. of water. The solution was neutralized with glacial acetic acid. The precipitate was removed by filtration with suction, washed with water and recrystallized from alcohol, whereby there was obtained 4'-(dimethylamino) 3',5'-dimethyl-2-(methylsulfonyl)-acetophenone having a melting point of 132°-133° C.

후처리

  1. additionA suspension of 24.5 g
  2. additionThen, it was treated with 16 g
  3. temperaturecooled
  4. dissolutiondissolved in 300 ml
  5. customThe precipitate was removed by filtration with suction
  6. washwashed with water
  7. customrecrystallized from alcohol

출처 및 근거

ORD 기록
ord-8146e085fd0f45e99b70fbcc4c1cc9f8
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04515948

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